EP3856700A1 - Verfahren zur herstellung eines carbon-keramischen formkörpers - Google Patents
Verfahren zur herstellung eines carbon-keramischen formkörpersInfo
- Publication number
- EP3856700A1 EP3856700A1 EP19779844.0A EP19779844A EP3856700A1 EP 3856700 A1 EP3856700 A1 EP 3856700A1 EP 19779844 A EP19779844 A EP 19779844A EP 3856700 A1 EP3856700 A1 EP 3856700A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- fibers
- carbon
- carbonizable
- molded body
- shaped body
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
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- 239000011159 matrix material Substances 0.000 claims abstract description 45
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- 239000010703 silicon Substances 0.000 claims abstract description 40
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 28
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 24
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 43
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- 229910052799 carbon Inorganic materials 0.000 claims description 38
- 238000003763 carbonization Methods 0.000 claims description 17
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- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 claims description 2
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- ILJSQTXMGCGYMG-UHFFFAOYSA-N triacetic acid Chemical compound CC(=O)CC(=O)CC(O)=O ILJSQTXMGCGYMG-UHFFFAOYSA-N 0.000 claims description 2
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- 239000002025 wood fiber Substances 0.000 claims description 2
- 210000002268 wool Anatomy 0.000 claims description 2
- 239000004952 Polyamide Substances 0.000 claims 1
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 6
- 229920003043 Cellulose fiber Polymers 0.000 description 5
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 5
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 description 5
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- 235000019837 monoammonium phosphate Nutrition 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 238000010000 carbonizing Methods 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
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- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000007833 carbon precursor Substances 0.000 description 2
- 239000000701 coagulant Substances 0.000 description 2
- 230000032798 delamination Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
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- 229910017053 inorganic salt Inorganic materials 0.000 description 2
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- 239000000843 powder Substances 0.000 description 2
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- 239000012266 salt solution Substances 0.000 description 2
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- 238000005475 siliconizing Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
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- DNIAPMSPPWPWGF-VKHMYHEASA-N (+)-propylene glycol Chemical compound C[C@H](O)CO DNIAPMSPPWPWGF-VKHMYHEASA-N 0.000 description 1
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- YPFDHNVEDLHUCE-UHFFFAOYSA-N 1,3-propanediol Substances OCCCO YPFDHNVEDLHUCE-UHFFFAOYSA-N 0.000 description 1
- UIDCSEZVSRDXDY-UHFFFAOYSA-N 2-ethyl-3-methyl-1h-imidazol-3-ium;acetate Chemical compound CC([O-])=O.CCC=1NC=C[N+]=1C UIDCSEZVSRDXDY-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- RAXXELZNTBOGNW-UHFFFAOYSA-O Imidazolium Chemical compound C1=C[NH+]=CN1 RAXXELZNTBOGNW-UHFFFAOYSA-O 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- NQRYJNQNLNOLGT-UHFFFAOYSA-O Piperidinium(1+) Chemical compound C1CC[NH2+]CC1 NQRYJNQNLNOLGT-UHFFFAOYSA-O 0.000 description 1
- RWRDLPDLKQPQOW-UHFFFAOYSA-O Pyrrolidinium ion Chemical compound C1CC[NH2+]C1 RWRDLPDLKQPQOW-UHFFFAOYSA-O 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
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- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical compound OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 description 1
- ZCQWOFVYLHDMMC-UHFFFAOYSA-O hydron;1,3-oxazole Chemical compound C1=COC=[NH+]1 ZCQWOFVYLHDMMC-UHFFFAOYSA-O 0.000 description 1
- SMWDFEZZVXVKRB-UHFFFAOYSA-O hydron;quinoline Chemical compound [NH+]1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-O 0.000 description 1
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- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
- C04B35/573—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained by reaction sintering or recrystallisation
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/636—Polysaccharides or derivatives thereof
- C04B35/6365—Cellulose or derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
- C04B35/83—Carbon fibres in a carbon matrix
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/0022—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof obtained by a chemical conversion or reaction other than those relating to the setting or hardening of cement-like material or to the formation of a sol or a gel, e.g. by carbonising or pyrolysing preformed cellular materials based on polymers, organo-metallic or organo-silicon precursors
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/4505—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application
- C04B41/4523—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application applied from the molten state ; Thermal spraying, e.g. plasma spraying
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5093—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with elements other than metals or carbon
- C04B41/5096—Silicon
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/24—Formation of filaments, threads, or the like with a hollow structure; Spinnerette packs therefor
- D01D5/247—Discontinuous hollow structure or microporous structure
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5216—Inorganic
- C04B2235/524—Non-oxidic, e.g. borides, carbides, silicides or nitrides
- C04B2235/5248—Carbon, e.g. graphite
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5252—Fibers having a specific pre-form
- C04B2235/5256—Two-dimensional, e.g. woven structures
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/616—Liquid infiltration of green bodies or pre-forms
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
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- C—CHEMISTRY; METALLURGY
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Definitions
- the invention relates to a method for producing a carbon-ceramic molded body which has a carbon fiber-reinforced carbon matrix and a content of silicon carbide and silicon.
- C / SiC silicon carbide in a carbon matrix
- C / C-SiC-Si carbon matrix contains carbon fibers (C / C) and also SiC and Si.
- the C / C composites are reacted with Si, whereby the known C / Si or C / C-SiC composites are obtained.
- the state of the art shows that the microstructure of the carbon precursor has an essential influence on the later properties of the C / C-SiC body.
- the microstructure can be determined by the matrix precursor, the fiber structure
- Segmentation cracks lead to a high conversion of the fibers to SiC and thus to poorer mechanical properties of the C / C-SiC body.
- the process for coating the fibers with SiC or pyrolytic carbon is known from the literature, which is very expensive and time-consuming (see Y. Cui, A. Li, B. Li, X. Ma, R. Bai, W. Zhang, M. Ren, "Microstructure and ablation mechanism of C / C-SiC composites", Journal of the European Ceramic Society, Vol. 34, pp. 171-177 (2014)).
- This coating of the fibers improves the fiber-matrix interface, so that a specifically adapted C / C microstructure with dense segments of fiber bundles is obtained.
- Additional materials such as polymer matrices, and / or additional
- carbonized molded body is then subjected to liquid siliconization to the carbon ceramic molded body.
- the cellulose is of natural origin or in the form of a carbonizable one
- Chemical pulp or carbonizable paper pulp is used. It is also advantageous if the degree of polymerization of the cellulose is optimized, preferably between approximately 108 and 5000, in particular between approximately 250 and 2000.
- the carbonizable fibers are carbonizable natural fibers and / or carbonizable chemical fibers and the carbonizable textile fabrics are based on the carbonizable natural fibers and / or carbonizable chemical fibers.
- the natural fibers are seed fibers, in particular cotton, bast fibers, in particular flax, hemp, jute, kinap, ramie,
- Abaca, Rosenna and / or Urena hard fibers, in particular alpha or espato grass, fique, henecen, coconut, manila, porphium and / or glisal,
- Natural substances of vegetable origin copper silk fibers, viscose fibers, modal fibers, rayon and cellulose acetate fibers, in particular as acetate or triacetate, alginate fibers, polyisoprene fibers or synthetic fibers, in particular elasto fibers, fluorofibers, polyacrylic fibers, in particular based on polyacrylonitrile or modacrylics, or aramid fibers, especially nylon, especially nylon, Represent polychloride fibers, in particular based on polyvinyl chloride and polyvinylidene chloride, polyester fibers, polyolefin fibers, in particular based on polyethylene and polypropylene, or polyvinyl alcohol fibers.
- Shaped body is between about 10 and 90 wt .-%, in particular between about 20 and 75 wt .-%.
- the carbonizable shaped body as the starting material of the process according to the invention is sheet-like, it being particularly preferred that several sheet-like shaped bodies are pressed together.
- the amount of cellulose is expediently about 2 to 30% by weight, in particular about 4 to 15% by weight, the solution system containing the cellulose, optionally with incorporated property-changing additives, mixed with a textile structure and this mixing system for coagulating the cellulose contained in the solution system in a
- Coagulation medium in particular introduced into an aqueous coagulation medium, and the shaped body formed by coagulation is washed and dried.
- the temperature of the molten ionic liquid is preferably set to less than approximately 160 ° C., in particular less than approximately 130 ° C., and / or to more than approximately 20 ° C., in particular more than approximately 30 ° C.
- the solution system has a zero viscosity (measured with a rotational viscometer) between approximately 2 and 1000 Pa.s, in particular between approximately 10 and 250 Pa.s. It is also considered advantageous if the coagulation medium is water,
- Monoalcohols in particular methanol, ethanol, propanol and / or butanol, contains polyhydric alcohols, in particular glycerol, ethylene glycol, diethylene glycol, triethylene glycol, 1,4-butanediol, 1,2-propanediol, 1,3-propanediol and / or 1,6-hexanediol, or mixtures of these coagulants. It is expedient here if the coagulation medium contains the coagulant in an amount of about 5 to 95% by weight, in particular about 20 to 80% by weight. It is particularly advantageous if the cellulose-containing one
- Solution system before mixing with the textile structures to about 10 to 140 ° C, in particular to about 40 to 120 ° C, and / or the coagulation medium to a temperature of about 20 to 90 ° C, in particular about 20 to 60 ° C. becomes.
- Shaped body a more extensive shaping in a heating press and / or by mechanical action, in particular cutting, or one
- the invention is not subject to any significant restrictions in the choice of the particular ionic liquid.
- it can be ionic liquids based on imidazolium, oxazolium, thiazolium, piperidinium, pyrrolidinium and quinolinium.
- the previously known shaped body from WO 2013098203 A2 (there claim 35) is further processed to a porous carbonized shaped body (C / C shaped body).
- the previously known shaped body is carbonized, in particular in an inert gas atmosphere.
- the carbonization takes place at a temperature between approximately 400 ° C. and 3000 ° C., in particular between approximately 700 ° C. and 2400 ° C.
- a heating rate between about 0.5 K / min and 10 K / min, in particular about 1 K / min and 5 K / min, is aimed for.
- the carbonized molded body shows a compact C / C structure with isolated pores in light microscopic images, which are formed in the molded body due to the pyrolysis products formed.
- the compactness of the carbon structure of the carbonized shaped body can be attributed to the high fiber-matrix adhesion.
- the C / C molded body according to the invention exhibits high fiber-matrix adhesion without thermoplastic or thermosetting plastics, without a previously carried out fiber finishing and thus no further process steps being necessary.
- Another advantage of this carbonized molded body is that the carbonization of the precursor fiber, corresponding to the cellulose fiber, is not carbonized beforehand, but the entire molded body
- Carbonization is subjected to in one piece, which saves another process step.
- the carbonized molded body has a carbon yield between about 10% and 40%, in particular from about 15% to 35%.
- Residual carbon content gives the person skilled in the art the possibility of finishing the textile structure with inorganic salt solutions.
- the inorganic solutions which are particularly advantageous in the context of the invention are phosphorus-containing salts, such as ammonium dihydrogen phosphate (ADHP), or salts of p-tosylate, such as ammonium p-tosylate. Equipping the textile structure before carbonization leads to an increase in the carbon yield, so that a carbonized one
- Shaped body with a residual carbon content of about 30% is obtained.
- the carbonization is preferably controlled so that a porosity of about 5 to 80%, in particular of about 20 to 55%, is established in the porous carbonized molded body. This control is achieved so that the
- Factors such as the solution system, in which the proportion of cellulose dissolved in a molten ionic liquid is varied, the duration of exposure of this solution system before it is removed by means of a coagulation medium and / or by the addition of inorganic salt solutions, which are used for finishing and thus serve to increase the carbon yield.
- the carbonization program can also be used for control.
- the process according to the invention is then continued by placing the porous carbonized shaped body in a container filled with silicon powder and / or silicon granules, in particular a graphite crucible, and in a vacuum and / or protective gas, in particular argon or nitrogen, up to a temperature above the silicon melting temperature is heated, the porous carbonized molded body being infiltrated with the liquid silicon via capillary forces and the silicon reacting with the carbon of the carbonized molded body. It is advantageous here that after the silicon has reacted with the carbon of the porous carbonized shaped body, the mixture is cooled, in particular by applying a vacuum.
- the method can also be used to the extent to which the porous carbonized molded body is infiltrated with liquid silicon. It has proven to be advantageous if the carbon-ceramic molded body has an increase in weight of approximately 30 to 140% by weight, in particular approximately 55 to 110% by weight, compared to the precursor in the form of the porous carbonized molded body.
- the last step of the invention is rounded off by the siliconization of the carbonized molded body.
- the siliconization with liquid silicon known in the prior art is used for this (see e.g. BD Nestler et al., In 6th International Kunststoff Chassis Symposium (Ed .: PE Pfeffer), Springer Vieweg, pp. 605-627 (2015)).
- the porous carbonized molded body to be iced which preferably must be completely penetrated by an open pore system, is used, for. B. placed in a graphite container, the bottom of which is filled with silicon powder and / or silicon granules. So-called wick technology has proven to be advantageous.
- the porous molded body to be siliconized is placed on a carbon body in the form of wicks, which have a very absorbent behavior with respect to the silicon.
- wicks are located partly in silicon powder and / or silicon granules, so that the liquid silicon can rise through the wick body and further infiltrate the molded body to be siliconized.
- these wick bodies there is no direct contact between the porous carbonized molded body to be siliconized and the liquid silicon, which has proven to be advantageous in that there is no complex removal of excess silicon from the siliconized carbon ceramic molded body. Due to the excellent wettability of the silicon against carbon, the crack system is infiltrated in the carbonized molded body by capillary forces.
- the silicon infiltrated in this way can thus react there with the matrix carbon to form silicon carbide.
- the conversion to silicon carbide serves as a diffusion barrier to the liquid silicon, so that the liquid silicon is prevented from penetrating further into the matrix up to the embedded carbon fiber reinforcement in order to also attack it.
- the porous carbonized molded body with liquid silicon in the temperature range from approximately 1450 ° C. to 2200 ° C., in particular between approximately 1600 ° C. and 1700 ° C. in a vacuum or
- infiltrated in inert gas in particular at temperatures of about 1400 ° C. to 2200 ° C., in particular from about 1500 ° C. to 2000 ° C.
- siliconization in vacuum it should preferably be ensured that residues of reactive gases are completely removed beforehand by flushing with inert gas.
- a fast heating rate can be selected here.
- the product of the process according to the invention in the form of the carbon-ceramic molded body has a large number of advantageous properties, such as a pore volume through which a fluid is accessible, of at most about 15% (according to DIN EN 1389: 2004-03), particularly preferably not more than about 12% and / or an elongation at break in the range of about 0.16% to 0.21% (according to DIN EN 658-3: 2002-11) and / or an apparent interlaminar shear strength of about 0.5 to 5 MPa (according to DIN EN 658-5: 2003-03), in particular from about 1 to 4 MPa.
- advantageous mechanical properties are in one
- Thermal protection system panel can be used.
- inexpensive cellulose as a reinforcing fiber in the process according to the invention and also as a matrix, the production costs are markedly reduced in comparison to those of the prior art processes. Thanks to the renewable bio-based raw material mentioned, the C0 2 balance can also be reduced.
- the non-carbonized reinforcing fibers are embedded in an organic matrix consisting of cellulose, so that chemical bonds can be formed due to the surface functionalities of the fibers and matrix, which strengthens the fiber-matrix adhesion.
- Carbonization step of the molded body consisting of in a matrix
- this improved fiber-matrix connection leads to this connection being additionally strengthened, since the fibers and the matrix are simultaneously carbonized. This simultaneous carbonization ensures that the carbon matrix perfectly surrounds the reinforcing fiber converted to carbon fiber. The siliconization in the last process step does not lead to the fact that the converted to carbon fiber
- Reinforcing fibers react with the liquid silicon to form silicon carbide.
- Si absorption of about 55% to 110% can be recorded for the carbon-ceramic shaped body according to the invention compared to 53% of the C / C-SiC shaped bodies according to the prior art.
- the carbon-ceramic matrix of the carbon-ceramic shaped body mainly consists of approximately 40 to 75% by weight of silicon carbide, in particular approximately 50 to 60% by weight, and also approximately 1 to 15% by weight of free silicon, preferably from about 2 to 11% by weight of free silicon, and preferably from about 20 to 60% by weight of carbon, in particular about 25 to 50% by weight
- Carbon matrix of the carbonized molded body converted to silicon carbide, which is particularly preferably not completely reacted to silicon carbide, but still consists of carbonized carbon matrix, whereby the mechanical
- Properties of the carbon-ceramic molded body can be advantageously influenced.
- the loss of mass and volume shrinkage influenced by the carbonization complete the crack structure in the fiber-reinforced carbonized molded body.
- the open porosity of the carbonized shaped body can be adjusted by the concentration of the matrix solution at the start of production. An open porosity in the range from about 15% to 60%, in particular from about 20% to 55%, can be achieved. The open porosity in the carbonized molded body further influences the
- a high open porosity in the carbon fiber-reinforced molded body leads to a high silicon absorption, which is possible up to 100%.
- existing carbon-ceramic molded body is in the range of about 5% to 13%, in particular from about 2% to 45%, which makes it very compact
- Example 1 The process according to the invention is started with the product which can be obtained by the process of WO 2013098203 A2.
- a cellulose fiber (further definition: commercially available tire cord fiber from the company Glanzstoff, lk Filêt, 1840 dtex) is wetted beforehand with a 6% solution of cellulose in ethyl-methylimidazolium acetate (EMIM acetate) on a metal mold with the dimensions 18 x 18 x 0.1 cm 3 so wet-wound that the metal mold is turned by 90 ° after four layers.
- the metal mold is rotated six times so that a 24-layer molded body is created. This 24-layer molded body is annealed at 70 ° C for 45 min.
- the ionic liquid (EMIM acetate) serving as solvent is washed out three times in an aqueous coagulation bath.
- the molded body is then dried in a heating press under a pressure of 6 N / cm 2 and at a temperature of 80 ° C. for 1 h.
- the carbonization takes place in a protective gas atmosphere in five steps: at the beginning the molded body is brought to 120 ° C with a heating rate of 10 K / min. After a holding time of 30 min, heating up to 200 ° C takes place at 5 K / min.
- the shrinking behavior is counteracted by further reducing the heating rate to 1 K / min to 260 ° C.
- the last increase in temperature to 1650 ° C occurs with a heating rate of 5 K / min.
- the carbon-ceramic molded body according to the invention has an open porosity of 6%, a flexural modulus of 4.7 MPa, a breaking strength of 20.1 MPa and an apparent interlaminar shear strength of 2.7 MPa.
- Example 1 Based on Example 1, a cellulose fiber is wetted beforehand by a solution consisting of an 8% solution of cellulose in EMIM acetate, on a metal mold with the dimensions 18 x 18 x 0.1 cm 3, so that a 24- layered molded body is formed. The subsequent process steps (washing, drying and carbonizing) are carried out as in Example 1 and lead to a carbonized molded body with a carbon yield of 22%.
- the fiber-reinforced carbon-ceramic molded body obtained has an open porosity of 11%, a flexural modulus of 8.1 MPa, a breaking strength of 18.2 MPa and an apparent interlaminar shear strength of 1.1 MPa.
- Example 1 As described in Example 1, a 24-layer molded article wound from cellulose is produced.
- the ionic liquid (EMIM acetate) serving as solvent is washed out three times in a coagulation bath consisting of an aqueous 0.4 M ADH P solution (ADHP: ammonium dihydrogen phosphate), while at the same time the shaped body is equipped with ADHP.
- the subsequent process steps (drying and carbonizing) are carried out as in Example 1 and lead to a carbonized molded body with a carbon yield of 31%. Siliconization is then carried out in accordance with the procedure of Example 1 in order to obtain the carbon-ceramic shaped body according to the invention.
- the fiber-reinforced carbon-ceramic molded body obtained has an open porosity of 6%, a flexural modulus of 11 MPa, a breaking strength of 45.1 MPa and an apparent interlaminar shear strength of 2.5 MPa.
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- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Structural Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Composite Materials (AREA)
- Inorganic Chemistry (AREA)
- Textile Engineering (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
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Abstract
Description
Claims
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DE102018123946.7A DE102018123946A1 (de) | 2018-09-27 | 2018-09-27 | Verfahren zur Herstellung eines Carbon-keramischen Formkörpers |
PCT/EP2019/076117 WO2020064972A1 (de) | 2018-09-27 | 2019-09-26 | Verfahren zur herstellung eines carbon-keramischen formkörpers |
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EP3856700A1 true EP3856700A1 (de) | 2021-08-04 |
EP3856700B1 EP3856700B1 (de) | 2023-04-19 |
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US (1) | US20220041511A1 (de) |
EP (1) | EP3856700B1 (de) |
CA (1) | CA3113883C (de) |
DE (1) | DE102018123946A1 (de) |
ES (1) | ES2949691T3 (de) |
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CN113788701B (zh) * | 2021-09-07 | 2022-12-02 | 华中科技大学 | 3d打印木质纤维素衍生碳化硅陶瓷的制备方法及产品 |
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US4396663A (en) * | 1979-06-11 | 1983-08-02 | The B. F. Goodrich Company | Carbon composite article and method of making same |
EP0519644B1 (de) * | 1991-06-17 | 1996-12-11 | General Electric Company | Siliziumcarbid-Verbundwerkstoff verstärkt mit Metallnitrid beschichteten Fasern |
JP3600642B2 (ja) * | 1993-09-02 | 2004-12-15 | ペーター ゲトケ | 反射体及びその製造方法 |
FR2734581B1 (fr) * | 1995-05-24 | 1997-08-14 | Europ Propulsion | Fil hybride pour la fabrication de preformes fibreuses de pieces en materiau composite et procede pour sa preparation |
US6503441B2 (en) * | 2001-05-30 | 2003-01-07 | General Electric Company | Method for producing melt-infiltrated ceramic composites using formed supports |
EP1284251B1 (de) | 2001-08-17 | 2011-09-28 | Eiji Tani | Poröses, leichtes und hitzebeständiges Strukturmaterial auf Siliciumkarbidbasis und Herstellungsverfahren dafür |
DE10161108A1 (de) * | 2001-12-12 | 2003-06-26 | Schunk Kohlenstofftechnik Gmbh | Verfahren zur Herstellung eines Keramikbauteils |
DE10348798A1 (de) | 2003-10-21 | 2005-06-16 | Papiertechnische Stiftung | Karbidische und oxidische Keramik und Verfahren zu ihrer Herstellung |
JP4475045B2 (ja) * | 2004-07-20 | 2010-06-09 | 三菱電機株式会社 | 反射鏡およびその製造方法 |
DE102005002633A1 (de) * | 2005-01-13 | 2006-07-20 | Deutsches Zentrum für Luft- und Raumfahrt e.V. | Verfahren und Vorrichtung zur Carbidbildner-Infiltration eines porösen kohlenstoffhaltigen Vorkörpers |
DE102006044848A1 (de) * | 2006-07-03 | 2008-01-10 | Deutsches Zentrum für Luft- und Raumfahrt e.V. | Verfahren zur Herstellung eines carbidkeramischen Kontaktkörpers und carbidkeramischer Kontaktkörper |
DE102006032636A1 (de) | 2006-07-13 | 2008-01-17 | Schunk Kohlenstofftechnik Gmbh | Verfahren zum Herstellen eines Keramiksubstrats sowie Keramiksubstrat |
DE102011122560B4 (de) * | 2011-12-29 | 2022-09-08 | Technikum Laubholz GmbH (TLH) | Textilverstärkter Formkörper, ein Verfahren zu dessen Herstellung sowie seine Verwendung |
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2018
- 2018-09-27 DE DE102018123946.7A patent/DE102018123946A1/de active Pending
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2019
- 2019-09-26 EP EP19779844.0A patent/EP3856700B1/de active Active
- 2019-09-26 CA CA3113883A patent/CA3113883C/en active Active
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- 2019-09-26 US US17/280,081 patent/US20220041511A1/en active Pending
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US20220041511A1 (en) | 2022-02-10 |
ES2949691T3 (es) | 2023-10-02 |
WO2020064972A1 (de) | 2020-04-02 |
CA3113883A1 (en) | 2020-04-02 |
CA3113883C (en) | 2023-02-14 |
PL3856700T3 (pl) | 2024-03-11 |
EP3856700B1 (de) | 2023-04-19 |
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